Methanol → HCID 178440154、化合物

HRID 1249552ノート

反応式

HRID 1249552 の反応式
[CH3:1][CH:2]([C:4]1[N:5]=[C:6]([C:17]([C:23]([F:26])([F:25])[F:24])([C:19]([F:22])([F:21])[F:20])[OH:18])[NH:7][C:8]=1[C:9]1[CH:14]=[CH:13][C:12](SC)=[CH:11][CH:10]=1)[CH3:3].O[O:28][S:29]([O-:31])=O.[K+].S(OOS([O-])(=O)=O)(O)(=O)=O.[K+].[CH3:44]O>>[CH3:1][CH:2]([C:4]1[N:5]=[C:6]([C:17]([C:23]([F:26])([F:24])[F:25])([C:19]([F:20])([F:21])[F:22])[OH:18])[NH:7][C:8]=1[C:9]1[CH:10]=[CH:11][C:12]([S:29]([CH3:44])(=[O:31])=[O:28])=[CH:13][CH:14]=1)[CH3:3]

参加物

5

反応物 4

HCID 887MethanolHCID 23690007Potassium hydrogen persulfateHCID 23707502Potassium hydroxy sulfiteHCID 178503127HCID 178503127、化合物

生成物 1

HCID 178440154HCID 178440154、化合物

実験手順

A mixture of 4.0 g (0.01 mole) of 4-(1-methylethyl)-5-(4-methylthiophenyl)-α,α-bis(trifluoromethyl)-1H-imidazole-2-methanol, 16.06 g (0.026 mole) of Oxone® (potassium hydrogen persulfate) and 115 ml of methanol was stirred at room temperature overnight. The inorganic solid was filtered off, and the filtrate was evaporated. The residue was partitioned between ethyl acetate and water. The layers were separated and the organic layer was washed with water, brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The product was recrystallized from dichloroethane affording 3.33 g (77%) of the title compound as a white solid, m.p. 182°-184° C.

後処理

  1. filtrationThe inorganic solid was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was partitioned between ethyl acetate and water
  4. customThe layers were separated
  5. washthe organic layer was washed with water, brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo
  8. customThe product was recrystallized from dichloroethane affording 3.33 g (77%) of the title compound as a white solid, m.p. 182°-184° C.

出典と根拠

ORDレコード
ord-b1c6dbbda2a349a497553983989702f1
出典データセット
uspto-grants-1986_12
特許番号
US04632930

反応ノート

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